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Co (II)&Ni (II) doped montmorillonite, and preparation method and application thereof

A technology of montmorillonite and donor, which is applied in the field of industrial catalysis and fine organic synthesis, can solve the problem that the oxidative property of cycloalkyl hydroperoxide is not fully utilized, the reaction conversion rate consumes the selectivity of oxidation products, and the reduction of cycloalkyl alcohol and Cycloalkyl ketone selectivity and other issues, to achieve the effect of inhibiting disordered diffusion, low cost, and high selectivity

Pending Publication Date: 2021-12-10
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the industrial catalytic oxidation of naphthenes is mainly based on homogeneous Co 2+ or Mn 2+ As a catalyst, oxygen (O 2 ) as an oxidizing agent, carried out at 150°C to 170°C, the main problems are high reaction temperature, low oxidation efficiency, poor selectivity of the target product, and the increase in reaction conversion will consume part of the selectivity of the oxidation product, especially the aliphatic di Acid production is difficult to suppress (Applied Catalysis A, General 2019,575:120-131; Catalysis Communications 2019,132:105809; Applied Catalysis A, General 2021,609:117904;)
The main causes of the above problems are: (1) O2 oxidation of cycloalkane in the industry mainly undergoes disordered free radical diffusion process; (2) oxidation intermediate products, cycloalkyl hydroperoxide and The free radical thermal decomposition path is converted to the target oxidation products cycloalkanol and cycloalkanone, which increases the uncontrollability of the reaction system and reduces the selectivity of cycloalkyl alcohol and cycloalkyl ketone; (3) the oxidation intermediate product, cycloalkyl The oxidation of hydrogen peroxide is not fully utilized; (4) the activity of cycloalkanol and cycloalkanone is higher than that of substrate cycloalkane
At present, there are no relevant reports on its application in the catalytic oxidation of naphthenes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 55

[0043] Example 55 is a scale-up experiment of Co(II) & Ni(II) doped montmorillonite catalyzed oxidation of cycloalkane.

Embodiment 1

[0045] Take 2.5968g (20.00mmol) anhydrous cobalt chloride, 1.2960g (10.00mmol) anhydrous nickel chloride and dissolve in 100mL distilled water, stir on a magnetic stirrer for 30min, and add 20.0g montmorillonite (can be The amount of the exchanged cation substance is 10 mmol), and stirred on a magnetic stirrer for 5.0 h. After standing for 30 minutes, filter, wash with water, dry in the shade at room temperature for 24.0 hours, and then vacuum-dry at 80°C. N 2 High temperature treatment at 700°C for 2.0h under atmosphere. Disperse the obtained montmorillonite-loaded material in 50.0 mL of dilute hydrochloric acid (2.0 mol / L), stir and wash for 6.0 h, filter under reduced pressure, rinse with 2×50 mL of deionized water until the pH value is 5.0-6.0, and dry in vacuum 12.3196g Co(II)&Ni(II) doped montmorillonite MT was obtained 1.0：2.0：1.0 -700-2.0 (the ratio of the amount of exchangeable cations, Co, and Ni substances is 1.0:2.0:1.0, 700 is the high temperature treatment tem...

Embodiment 2

[0047] Take 2.5920g (20.00mmol) of anhydrous nickel chloride and 1.3445g (10.00mmol) of anhydrous copper chloride and dissolve them in 100mL of distilled water, stir on a magnetic stirrer for 30min, and add 20.0g of montmorillonite (can be The amount of the exchanged cation substance is 10 mmol), and stirred on a magnetic stirrer for 5.0 h. After standing for 30 minutes, filter, wash with water, dry in the shade at room temperature for 24.0 hours, and then vacuum-dry at 80°C. N 2 High temperature treatment at 700°C for 2.0h under atmosphere. Disperse the obtained montmorillonite-loaded material in 50.0 mL of dilute hydrochloric acid (2.0 mol / L), stir and wash for 6.0 h, filter under reduced pressure, rinse with 2×50 mL of deionized water until the pH value is 5.0-6.0, and dry in vacuum 13.1983g Co(II)&Ni(II) doped montmorillonite MT-0 was obtained 1.0：2.0：1.0 -700-2.0 (the ratio of exchangeable cations, Ni, and Cu is 1.0:2.0:1.0, 700 is the high temperature treatment temper...

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Abstract

The invention relates to Co (II)&Ni (II) doped montmorillonite, a preparation method thereof and application of the Co (II)&Ni (II) doped montmorillonite in catalytic oxidation of naphthenic hydrocarbon to synthesize naphthenic alcohol and naphthenic ketone, and belongs to the field of industrial catalysis and fine organic synthesis. The method comprises the following steps: dispersing montmorillonite in a mixed aqueous solution of Co (II) salt and Ni (II) salt (the total amount is 30.0 mmol), stirring and loading metal ions, collecting a solid, carrying out high-temperature treatment, and carrying out post-treatment to obtain Co (II)&Ni (II) doped montmorillonite. The obtained Co (II)&Ni (II) doped montmorillonite is applied to catalysis of naphthenic hydrocarbon to obtain products naphthenic alcohol and naphthenic ketone. The catalytic reaction has the advantages of high selectivity of naphthenic alcohol and naphthenic ketone, low reaction temperature, few byproducts, small environmental influence and the like. In addition, the content of naphthenic hydroperoxide is low, and the safety coefficient is high. The invention provides an efficient, feasible and safe method for synthesizing naphthenic alcohol and naphthenic ketone through selective catalytic oxidation of naphthenic hydrocarbon.

Description

technical field [0001] The invention relates to a Co(II)&Ni(II) doped montmorillonite, a preparation method thereof and its application in catalytic oxidation of cycloalkane to synthesize cycloalkanol and cycloalkanone, belonging to the field of industrial catalysis and fine organic synthesis. Background technique [0002] Catalytic oxidation of naphthenes is a very important conversion process in the chemical industry. The oxidation products cycloalkanol and cycloalkanone are not only important organic solvents, but also important fine chemical intermediates, widely used in pesticides, medicines, dyes, surface Synthesis of fine chemical products such as active agents and resins, especially the production of polyamide fibers nylon-6 and nylon-66. At present, the industrial catalytic oxidation of naphthenes is mainly based on homogeneous Co 2+ or Mn 2+ As a catalyst, oxygen (O 2 ) as an oxidizing agent, carried out at 150°C to 170°C, the main problems are high reaction tem...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J37/30B01J37/08B01J21/16C07C45/33C07C49/395C07C49/403C07C49/413C07C29/50C07C35/06C07C35/20C07C35/08C07C35/205
CPCB01J23/755B01J37/30B01J37/08B01J21/16C07C45/33C07C29/50C07C2601/14C07C2601/18C07C2601/08C07C2601/20B01J35/394C07C49/395C07C49/403C07C49/413C07C35/06C07C35/20C07C35/08C07C35/205
Inventor 沈海民秦嘉伟
Owner ZHEJIANG UNIV OF TECH